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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 397 records · Page 22

Porous and Amorphous Mn x Mo 3 S 13 Chalcogel Electrode for High-Capacity Conversion-Based Lithium-Ion Batteries

While Li-ion batteries (LIBs) are a leading energy storage technology, their energy densities are limited by the low capacity of conventional intercalation cathodes, driving interest in high energy-density Li–S batteries that make use of conversion chemistry. Achieving high capacity, reversibility, and cycle stability, and controlling volume changes in conversion batteries during the charge–discharge process, however, remains challenging. Here, in this study, we present a porous, amorphous, sulfide-based Mn x Mo 3 S 13 chalcogel, which concurrently offers high capacity and cycle stability. The solution-processable room temperature synthesized Mn x Mo 3 S 13 (x = 0.25) chalcogel exhibits a local structure that resembles the Mo 3 S 13 cluster with Mn 2+ distributed across the Mo 3 S 13 matrix, as determined by synchrotron X-ray pair distribution function (PDF) and extended X-ray absorption fine structure (EXAFS). Ab initio molecular dynamics (AIMD) simulations reveal that Mn 2+ incorporation shortens the polysulfide chain in the gel matrix compared to the Mo 3 S 13 chalcogel, while forming a coordination environment with disulfide groups, analogous to the experimental findings. A Li/Mn 0.25 Mo 3 S 13 half-cell delivers 897 mAh g –1 capacity during the first discharge and retains 571 mAh g –1 capacity after 100 cycles at a C/3 rate. Distribution of relaxation time (DRT) unveils a stable solid–electrolyte interphase (SEI) formation upon cycling that enables charge–discharge reversibility. Here, the enhanced capacity retention and cycle stability compared to those of the Li/Mo 3 S 13 cell are attributed to the reduced dissolution of active mass into the electrolyte, facilitated by the formation of shorter polysulfide chains within the Mn 0.25 Mo 3 S 13 structure and the strong affinity of Lewis-acidic Mn 2+ for polysulfide anions generated during the charge–discharge process of the Li/Mn 0.25 Mo 3 S 13 cell. Thus, this work illustrates a design principle of material for high-capacity and cycle-stable Li-metal sulfide batteries.

25 ENERGY STORAGE↗

Gamma Radiation Effects in Amorphous and Crystalline Polyaryletherketones

This work investigates the effect of gamma radiation on chain scission and crosslinking in polyaryletherketone (PAEK) thermoplastic filaments, namely, polyetheretherketone (PEEK) and polyetherketoneketone (PEKK) that is either semicrystalline (PEKK-c) or highly amorphous (PEKK-a). The PAEK thermoplastic filaments were exposed to total ionizing doses (TID) of gamma radiation from 1 to 8 MGy in the Gamma Irradiation Facility at Sandia National Laboratories. A combination of thermal and FT-IR spectral analysis of the irradiated specimens was used to study the chain scission and crosslinking behavior between PEEK, PEKK-c, and PEKK-a. Crystallinity decreased with increased TID and melt enthalpy decreased. Despite clear indications of changes to melt and crystallization behavior, any change to the glass-transition temperature was minor until a post-irradiation thermal annealing occurred, which caused an increase in crystallinity. Gamma radiation impacted PEKK-a more due to the lower degree of initial crystallinity, where a reduction in melt enthalpy, crystallinity, and crystallization kinetics was observed. Despite these effects, the ability to achieve a higher degree of crystallization (X c < 20%) by annealing was not affected. The results presented here provide important insight into the performance of a class of commercialized PEKK thermoplastics exposed to a harsh radiation environment.

Crystallinity↗

Predicting orientation-dependent plastic susceptibility from static structure in amorphous solids via deep learning

It has been a long-standing materials science challenge to establish structure-property relations in amorphous solids. Here we introduce a rotationally non-invariant local structure representation that enables different predictions for different loading orientations, which is found essential for high-fidelity prediction of the propensity for stress-driven shear transformations. This novel structure representation, when combined with convolutional neural network (CNN), a powerful deep learning algorithm, leads to unprecedented accuracy for identifying atoms with high propensity for shear transformations (i.e., plastic susceptibility), solely from the static structure in both two- and three-dimensional model glasses. The data-driven models trained on samples at one composition and a given processing history are found transferrable to glass samples with different processing histories or at different compositions in the same alloy system. Our analysis of the new structure representation also provides valuable insight into key atomic packing features that influence the local mechanical response and its anisotropy in glasses.

36 MATERIALS SCIENCE↗

Eliminating chemo-mechanical degradation of lithium solid-state battery cathodes during >4.5 V cycling using amorphous Nb2O5 coatings

Abstract Lithium solid-state batteries offer improved safety and energy density. However, the limited stability of solid electrolytes (SEs), as well as irreversible structural and chemical changes in the cathode active material, can result in inferior electrochemical performance, particularly during high-voltage cycling (>4.3 V vs Li/Li + ). Therefore, new materials and strategies are needed to stabilize the cathode/SE interface and preserve the cathode material structure during high-voltage cycling. Here, we introduce a thin (~5 nm) conformal coating of amorphous Nb 2 O 5 on single-crystal LiNi 0.5 Mn 0.3 Co 0.2 O 2 cathode particles using rotary-bed atomic layer deposition (ALD). Full cells with Li 4 Ti 5 O 12 anodes and Nb 2 O 5 -coated cathodes demonstrate a higher initial Coulombic efficiency of 91.6% ± 0.5% compared to 82.2% ± 0.3% for the uncoated samples, along with improved rate capability (10x higher accessible capacity at 2C rate) and remarkable capacity retention during extended cycling (99.4% after 500 cycles at 4.7 V vs Li/Li + ). These improvements are associated with reduced cell polarization and interfacial impedance for the coated samples. Post-cycling electron microscopy analysis reveals that the Nb 2 O 5 coating remains intact and prevents the formation of spinel and rock-salt phases, which eliminates intra-particle cracking of the single-crystal cathode material. These findings demonstrate a potential pathway towards stable and high-performance solid-state batteries during high-voltage operation.

Science & Technology - Other Topics↗

Amorphous nickel hydroxide shell tailors local chemical environment on platinum surface for alkaline hydrogen evolution reaction

In analogy to natural enzymes, an elaborated design of catalytic systems with a specifically tailored local chemical environment could substantially improve reaction kinetics, effectively combat catalyst poisoning effect and boost catalyst lifetime under unfavourable reaction conditions. Here we report a unique design of ‘Ni(OH) 2 -clothed Pt-tetrapods’ with an amorphous Ni(OH) 2 shell as a water dissociation catalyst and a proton conductive encapsulation layer to isolate the Pt core from bulk alkaline electrolyte while ensuring efficient proton supply to the active Pt sites. This design creates a favourable local chemical environment to result in acidic-like hydrogen evolution reaction kinetics with a lowest Tafel slope of 27 mV per decade and a record-high specific activity and mass activity in alkaline electrolyte. The proton conductive Ni(OH) 2 shell can also effectively reject impurity ions and retard the Oswald ripening, endowing a high tolerance to solution impurities and exceptional long-term durability that is difficult to achieve in the naked Pt catalysts. Furthermore, the markedly improved hydrogen evolution reaction activity and durability in an alkaline medium promise an attractive catalyst material for alkaline water electrolysers and renewable chemical fuel generation.

36 MATERIALS SCIENCE↗

Revealing key structures for reversible sulfur redox in amorphous polymeric sulfur

Amorphous polymeric sulfur cathodes, such as sulfurized polyacrylonitrile (SPAN), enable high-energy lithium-sulfur batteries without cobalt or nickel, leveraging abundant sulfur. However, the limited in situ understanding of their synthesis and electrochemistry has impeded targeted optimization. Here, in this study, we integrate operando high-energy total scattering with sulfur K-edge X-ray absorption spectroscopy to monitor SPAN's formation and cycling in real time. Our results show that S-C bond formation halts further fusion of cyclized polyacrylonitrile, fostering π-π stacking and a transition from long-chain to short-chain sulfur-critical for reversible sulfur redox. These features synergistically minimize polysulfide dissolution and charge-transfer resistance, enabling optimized SPAN to achieve high capacity retention over 1,000 cycles. Operando X-ray absorption spectroscopy reveals that residual protons drive thiol-thione tautomerism, with lithium replacement during the first discharge causing ~20% irreversible capacity loss. To enhance performance, minimizing -NH groups and expanding pyridine networks are key. These findings transform SPAN optimization from empirical tuning to mechanism‑guided engineering and point the way towards sulfur loadings and energy densities competitive with state‑of‑the‑art Li‑ion cathodes.

25 ENERGY STORAGE↗

Integration of amorphous ferromagnetic oxides with multiferroic materials for room temperature magnetoelectric spintronics

A room temperature amorphous ferromagnetic oxide semiconductor can substantially reduce the cost and complexity associated with utilizing crystalline materials for spintronic devices. We report a new material (Fe 0.66 Dy 0.24 Tb 0.1 ) 3 O 7-x (FDTO), which shows semiconducting behavior with reasonable electrical conductivity (~500 mOhm-cm), an optical band-gap (2.4 eV), and a large enough magnetic moment (~200 emu/cc), all of which can be tuned by varying the oxygen content during deposition. Magnetoelectric devices were made by integrating ultrathin FDTO with multiferroic BiFeO 3 . A strong enhancement in the magnetic coercive field of FDTO grown on BiFeO 3 validated a large exchange coupling between them. Additionally, FDTO served as an excellent top electrode for ferroelectric switching in BiFeO3 with no sign of degradation after ~10 10 switching cycles. RT magneto-electric coupling was demonstrated by modulating the resistance states of spin-valve structures using electric fields.

36 MATERIALS SCIENCE↗

Kinetic analyses for solid-state phase transition of metastable amorphous-AlO x (2.5 < x ≤ 3.0) nanostructures into crystalline alumina polymorphs

Solid-solid phase change materials (SS-PCMs) hold promise for energy storage/dissipation in batteries and energetic materials. Yet, phase change kinetics for SS-PCMs undergoing metastable to semi-stable/stable phase transformations remain relatively ill-studied because trapping metastable phases remain challenging. Recently, we demonstrated the kinetic entrapment and stabilization of a highly disordered and amorphous Al-oxide phase m-AlO x @C (x~2.5-3.0) via laser ablation synthesis in solution (LASiS). We report here, to our knowledge, the first chemical kinetics analysis for S-S phase transition of the m-AlO 3 @C nanocomposites (< 5–8 nm sizes) into semi-stable equilibrium alumina phases (θ/γ-Al 2 O 3 ) via disproportionation reaction, while releasing excess trapped gases. Our results indicate the atomic density of the AlO 3 structures to be ~5–10 times less than that of the final Al 2 O 3 phases, which led to the hypothesis of a volume shrinkage process during their phase transition. Temperature-dependent X-ray diffraction studies reveal the high-temperature phase transition for m-AlO 3 → θ/γ-Al 2 O 3 to follow contracting volume kinetics model, thereby validating our earlier hypothesis. Using the geometric volume contraction model, reaction kinetics analyses from Arrhenius plots reveal the activation energy barrier for the phase transition to be ~270±11 kJ/mol. This makes the activation energy barrier nearly identical to the oxidation of micron-sized Al particles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ultrasmall amorphous zirconia nanoparticles catalyse polyolefin hydrogenolysis

Carbon–carbon bond cleavage reactions, adapted to deconstruct aliphatic hydrocarbon polymers and recover the intrinsic energy and carbon value in plastic waste, have typically been catalysed by metal nanoparticles or air-sensitive organometallics. Metal oxides that serve as supports for these catalysts are typically considered to be inert. Here we show that Earth-abundant, non-reducible zirconia catalyses the hydrogenolysis of polyolefins with activity rivalling that of precious metal nanoparticles. To harness this unusual reactivity, our catalytic architecture localizes ultrasmall amorphous zirconia nanoparticles between two fused platelets of mesoporous silica. Macromolecules translocate from bulk through radial mesopores to the highly active zirconia particles, where the chains undergo selective hydrogenolytic cleavage into a narrow, C18-centred distribution. Calculations indicated that C–H bond heterolysis across a Zr–O bond of a Zr(O) 2 adatom model for unsaturated surface sites gives a zirconium hydrocarbyl, which cleaves a C–C bond via β-alkyl elimination.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Spin-on deposition of amorphous zeolitic imidazolate framework films for lithography applications

Amorphous zeolitic imidazolate framework (aZIF) films have been recently introduced as resists for electron beam and extreme ultraviolet lithography. aZIFs are also being considered for separation applications, including thin film membranes. However, the reported methods for aZIF deposition are currently based on highly empirical trial-and-error approaches that hinder control of film composition, thickness and uniformity as well as scale-up and transferability to different coating geometries. This work presents a method for depositing aZIF films with controllable thickness using dilute precursors mixed immediately before encountering the substrate. Importantly, the method is amenable to quantitative analysis by computational fluid dynamics to extract intrinsic deposition rates and limiting reactant transport diffusivities, enabling predictive physics-based modeling of the deposition process. This allows the deposition method to be adapted for spin coating on silicon wafers to prepare high-quality aZIF films with consistently controlled thickness. Using this approach, high-resolution resist performance and wafer-scale use for beyond extreme-ultraviolet lithography of aZIF films is demonstrated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Low temperature and limited water activity reveal a pathway to magnesite via amorphous magnesium carbonate

Forsterite carbonated in thin H 2 O films to magnesite via amorphous magnesium carbonate during reaction with H 2 O-bearing liquid CO 2 at 25 °C. This novel reaction pathway contrasts with previous studies that were carried out at higher H 2 O activity and temperature, where more highly hydrated nesquehonite was the metastable intermediate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structural evolution of amorphous calcium sulfate nanoparticles into crystalline gypsum phase

The involvement of amorphous calcium sulfate (ACS) as a precursor to calcium sulfate crystallization remains an important but poorly understood phenomenon, especially the mechanism by which ACS evolves into crystalline phase. In this study, we captured the ACS nanoparticles as a precursor to calcium sulfate crystallization in a concentrated CaCl 2 solution at 90 °C and observed several stages of its evolution. The ACS nanoparticles grew by simultaneous fusion and internal structural evolution. Aggregation of the ACS nanoparticles gave birth to bulk ACS particles within which nanocrystalline domains sprouted and developed into crystalline gypsum. This work deepens the understanding of the evolution of ACS nanoparticles and its role in multistage crystallization of calcium sulfate.

36 MATERIALS SCIENCE↗

Failure modes of protection layers produced by atomic layer deposition of amorphous TiO 2 on GaAs anodes

Amorphous titanium dioxide (a-TiO 2 ) films formed by atomic layer deposition can serve as protective coatings for semiconducting photoanodes in water-splitting cells using strongly alkaline aqueous electrolytes. Herein, we experimentally examine the mechanisms of failure for p + -GaAs anodes coated with a-TiO 2 films (GaAs/a-TiO 2 ). Galvanic displacement of exposed GaAs by Au allowed imaging of pinholes in the a-TiO 2 coatings, and enabled collection of quantitative and statistical data associated with pinhole defects. A combination of imaging, electrochemical measurements, and quantitative analyses of corrosion products indicated that extrinsic pinholes were present in the a-TiO 2 films before electrochemical operation. During electrochemical operation these pinholes led to pitting corrosion of the underlying GaAs substrate. The dominant source of pinholes was the presence of atmospheric particulate matter on the GaAs surface during deposition of the a-TiO 2 layer. The pinhole density decreased substantially when the thickness of the a-TiO 2 coating increased beyond 45 nm, and approached zero when the thickness of the film exceeded 112 nm. The density of pinholes in films thinner than 45 nm decreased when the a-TiO 2 coating was deposited in an environmentally controlled cleanroom. Pinhole-free GaAs/a-TiO 2 devices were also tested via chronoamperometry to quantify the rate of pinhole formation during electrochemistry. The time-to-failure increased with thickness, suggesting that the failure mechanism may involve diffusion or migration through the film. However, other mechanisms may also contribute to the degradation of thicker films (>112 nm). Nevertheless, as previously hypothesized, extrinsic pinhole defects formed during deposition and testing control the short-term protective performance of the a-TiO 2 film for GaAs anodes evolving O 2 from water.

25 ENERGY STORAGE↗

Understanding, quantifying, and controlling the molecular ordering of semiconducting polymers: from novices to experts and amorphous to perfect crystals

Molecular packing and texture of semiconducting polymers are often critical to the performance of devices using these materials. Although frameworks exist to quantify the ordering, interpretations are often just qualitative, resulting in imprecise use of terminology. Here, we reemphasize the significance of quantifying molecular ordering in terms of degree of crystallinity (volume fractions that are ordered) and quality of ordering and their relation to the size scale of an ordered region. We are motivated in part by our own imprecise and inconsistent use of terminology in the past, as well as the need to have a primer or tutorial reference to teach new group members. We strive to develop and use consistent terminology with regards to crystallinity, semicrystallinity, paracrystallinity, and related characteristics. To account for vastly different quality of ordering along different directions, we classify paracrystals into 2D and 3D paracrystals and use paracrystallite to describe the spatial extent of molecular ordering in 1–10 nm. We show that a deeper understanding of molecular ordering can be achieved by combining grazing-incidence wide-angle X-ray scattering and differential scanning calorimetry, even though not all aspects of these measurements are consistent, and some classification appears to be method dependent. We classify a broad range of representative polymers under common processing conditions into five categories based on the quantitative analysis of the paracrystalline disorder parameter (g) and thermal transitions. A small database is presented for 13 representative conjugated and insulating polymers ranging from amorphous to semi-paracrystalline. Lastly, we outline the challenges to rationally design more perfect polymer crystals and propose a new molecular design approach that envisions conceptual molecular grafting that is akin to strained and unstrained hetero-epitaxy in classic (compound) semiconductors thin film growth.

36 MATERIALS SCIENCE↗

Understanding methanol dissociative adsorption and oxidation on amorphous oxide films

Interactions between a transition metal (oxide) catalyst and a support can tailor the number and nature of active sites, for instance in the methanol oxidation reaction.In this report we use ambient pressure X-ray photoelectron spectroscopy (AP-XPS) to identify and compare the surface adsorbates that form on amorphous metal oxide films that maximize such interactions. Considering Al (1−x) M x O y (M = Fe or Mn) films at a range of methanol : oxygen gas ratios and temperatures, we find that the redox-active transition metal site (characterized by methoxy formation) dominates dissociative methanol adsorption, while basic oxygen sites (characterized by carbonate formation) play a lesser role. Product detection, however, indicates complete oxidation to carbon dioxide and water with partial oxidation products (dimethyl ether) comprising a minor species. Comparing the intensity of methoxy and hydroxyl features at a fixed XPS chemical shift suggests methanol deprotonation during adsorption in oxygen rich conditions for high transition metal content. However, increasing methanol partial pressure and lower metal site density may promote oxygen vacancy formation and the dehydroxylation pathway, supported by a nominal reduction in the oxidation state of iron sites. These findings illustrate that AP-XPS and mass spectrometry together are powerful tools in understanding metal–support interactions, quantifying and probing the nature of catalytic active sites, and considering the link between electronic structure of materials and their catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Experimentally informed structure optimization of amorphous TiO 2 films grown by atomic layer deposition

Amorphous titanium dioxide TiO 2 (a-TiO 2 ) has been widely studied, particularly as a protective coating layer on semiconductors to prevent corrosion and promote electron–hole conduction in photoelectrochemical reactions. The stability and longevity of a-TiO 2 is strongly affected by the thickness and structural heterogeneity, implying that understanding the structure properties of a-TiO 2 is crucial for improving the performance. This study characterized the structural and electronic properties of a-TiO 2 thin films (~17 nm) grown on Si by atomic layer deposition (ALD). Fluctuation spectra V(k) and angular correlation functions were determined with 4-dimensional scanning transmission electron microscopy (4D-STEM), which revealed the distinctive medium-range ordering in the a-TiO 2 film. A realistic atomic model of a-TiO 2 was established guided by the medium-range ordering and the previously reported short-range ordering of a-TiO 2 film, as well as the interatomic potential. The structure was optimized by the StructOpt code using a genetic algorithm that simultaneously minimizes energy and maximizes the match to experimental short- and medium-range ordering. The StructOpt a-TiO 2 model presents improved agreements with the medium-range ordering and the k-space location of the dominant 2-fold angular correlations compared with a traditional melt-quenched model. The electronic structure of the StructOpt a-TiO 2 model was studied by ab initio calculations and compared to the crystalline phases and experimental results. Finally, this work uncovered the medium-range ordering in a-TiO 2 thin films and provided a realistic a-TiO 2 structure model for further investigation of structure–property relationships and materials design. In addition, the improved multi-objective optimization package StructOpt was provided for structure determination of complex materials guided by experiments and simulations.

36 MATERIALS SCIENCE↗